CN102397300A - Extraction method of phlorotannins - Google Patents
Extraction method of phlorotannins Download PDFInfo
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- CN102397300A CN102397300A CN2010102779021A CN201010277902A CN102397300A CN 102397300 A CN102397300 A CN 102397300A CN 2010102779021 A CN2010102779021 A CN 2010102779021A CN 201010277902 A CN201010277902 A CN 201010277902A CN 102397300 A CN102397300 A CN 102397300A
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- brown algae
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- algae polyphenol
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Abstract
The invention provides an extraction method of phlorotannins, comprising the following steps: pretreating raw materials, leaching, cooling, washing, adsorbing with resin, eluting, and freeze drying. According to the invention, the advantages of high yield, low cost, convenient for industrial production and the like can be achieved.
Description
Technical field
The present invention relates to the marine organisms field, particularly a kind of method of from the Brown algae biology, extracting the Brown algae polyphenol.
Background technology
The Brown algae polyphenol extensively is present in the sea-plant Brown algae, and it is construction unit with the benzenetriol, mainly is divided into oligomerization phloroglucinol and Eckol class polyphenol.Research proof Brown algae polyphenol has anti-cardiovascular disease, antibiotic, antiviral, dissolve algae, antioxidation, anti-diabetic syndrome, protect the liver and suppress wide biological activity such as lysyl oxidase hyaluronidase.The Brown algae polyphenol has structure and the activity that is different from the land plant polyphenol, is the natural materials of one type of uniqueness.
Have at present the method for distilling about the Brown algae polyphenol of report mainly adopt alcoholic solution room temperature lucifuge extract crude extract, obtain Brown algae polyphenol extract through steps such as organic solvent washing, distilling under reduced pressure then.But the product that these methods obtain has caffeine, alkaloid is higher, and therefore shortcomings such as Product Safety is low, length consuming time are unfavorable for suitability for industrialized production.
Summary of the invention
In view of this, the purpose of this invention is to provide a kind of method for distilling of Brown algae polyphenol, compare, have that purity height, yield are high, production cost is low, help the characteristics of suitability for industrialized production with method in the document.
The present invention adopts following technical scheme: as raw material, carry out the operation of following steps with the biomaterial that contains the Brown algae polyphenol:
Pretreatment of raw material: take by weighing the biological raw material that contains the Brown algae polyphenol of certain quantity of fresh, remove precipitate, phytoplankton and other attachment, rinse well repeatedly, dry, carry out fragmentation with tap water;
Leaching: with the antioxidant of the biomaterial after the fragmentation by weight in wet base adding 0.002～0.02%; With the aqueous solution that contains organic solvent 50～90% by 1: 2～9 mixed; Fully stir to be placed on and handle 3～6min in the ultrasound wave; Put into 40～80 ℃ of waters bath with thermostatic control, vibration, lucifuge leaching 1～6 hour, separate supernatant, organic solvent is removed in distilling under reduced pressure;
Cooling washing: will leach back solution and place 0～4 ℃ of refrigerator static 2～8 hours, separate supernatant, using volume ratio is that 1: 1～4 aqueous solutions of organic solvent wash supernatant, organic solvent is removed in distilling under reduced pressure;
Absorption: the solution that above-mentioned steps is obtained adsorbs with macroporous resin, adsorb saturated after, use the 2BV distilled water wash;
Eluting: the eluant with containing 50～85% organic solvents carries out the eluting desorbing, and collects target product;
Lyophilization: target product obtains finished product Brown algae polyphenol after lyophilization.
The said biomaterial that contains the Brown algae polyphenol contains the thread of brown pigment or the thalloid algae of silk in life Yu Haiyang or the fresh water.
The said biomaterial that contains the Brown algae polyphenol is Sargassum Brown algae or Larminaria plant.
The antioxidant that adds in the said leaching step is a butylated hydroxyarisol (BHA), 2, one or more in 6-di-t-butyl hydroxy-methylbenzene (BHT), sodium sulfite, sodium sulfite, sodium pyrosulfite, the sodium thiosulfate.
The organic solvent of using in the said leaching step is one or more in acetone, methanol, toluene, ethanol, ethyl acetate, chloroform, the petroleum ether.
The separation method of supernatant is siphon, centrifugal, in filtering one or more in the said leaching step.
The organic solvent of using in the said cooling washing step is one or more in acetone, methanol, toluene, ethanol, ethyl acetate, chloroform, the petroleum ether.
Organic solvent in the said elution step is one or more in ethanol, acetone, methanol, toluene, ethyl acetate, the chloroform.
The Brown algae polyphenol finished product of said final acquisition is solid-state or liquid.
The Brown algae polyphenol finished product of said final acquisition is solid-state.
The NaCl that also often adds trace in the solution of using in the leaching process, (NH
4)
2SO
4, salts such as KCl are used for the effect strengthening leaching; After for the first time the supernatant leaching being finished, filtering residue repeats lixiviate once again, merges extracted twice liquid vacuum rotary steam and removes organic solvent.
The present invention compares with existing method, has the following advantages: (1) the present invention at first adopts organic solvent slightly to extract polyphenol, and product purity, the relative water extraction method of extraction ratio are improved, and the relative water extraction method of the degree of oxidation of product is lower; (2) the leaching step has added a certain amount of antioxidant among the present invention, has prevented the oxidation of Brown algae polyphenol effectively; (3) adopt macroporous resin to carry out adsorbing separation after slightly carrying, this method is simple, and is easy to operate, and energy consumption is lower, and operating condition is gentle, has avoided the effective ingredient inactivation, and product yield and purity usury are in industrialization, large-scale production.In sum, the present invention has the yield height, production cost is low, is beneficial to the characteristics of suitability for industrialized production.
The specific embodiment
Describe in conjunction with specific embodiment.
Embodiment 1
Carry out the extraction of Brown algae polyphenol through following steps:
The first step: take by weighing the fresh Thallus Laminariae (Thallus Eckloniae) of 1000g, remove precipitate, phytoplankton and other attachment, rinse well repeatedly with tap water then, in 105 ℃ of baking ovens, dry to constant weight, obtain solid content and be about 100g, smash the refiner fragmentation to pieces with tissue;
Second step: the biological raw material after the fragmentation is added 0.002% butylated hydroxyarisol (BHA) by weight in wet base; With the mixed of the aqueous solution that contains ethanol 70% by 1: 2; Fully stir to be placed on and handle 3min in the ultrasound wave; Put into 60 ℃ of waters bath with thermostatic control, vibration, lucifuge leaching 1 hour, separation of supernatant, organic solvent is removed in distilling under reduced pressure;
The 3rd step: placed 4 ℃ of refrigerators static 8 hours, separate supernatant, using volume ratio is 1: 1 chloroform water solution washing supernatant, organic solvent is removed in distilling under reduced pressure;
The 4th the step: adsorb with macroporous resin, adsorb saturated after, use the 2BV distilled water wash;
The 5th step: carry out the eluting desorbing with containing 85% alcoholic acid eluant, and collect target product;
The 6th step: target product obtains 0.03g Brown algae polyphenol solid after lyophilization, productive rate is 0.3 ‰.
Embodiment 2
Carry out the extraction of Brown algae polyphenol through following steps:
The first step: take by weighing the fresh Thallus Sargassi Kjellmaniani of 1000g, remove precipitate, phytoplankton and other attachment, rinse well repeatedly with tap water then, in 105 ℃ of baking ovens, dry to constant weight, obtain solid content and be about 50g, smash the refiner fragmentation to pieces with tissue;
Second step: biological raw-material with after the fragmentation by 2 of weight in wet base adding 0.02%; 6-di-t-butyl hydroxy-methylbenzene (BHT); With the mixed of the aqueous solution that contains acetone 80% by 1: 4, fully stir to be placed on and handles 6min in the ultrasound wave, put into 40 ℃ of waters bath with thermostatic control, vibration, lucifuge leaching 2 hours; Separation of supernatant, organic solvent is removed in distilling under reduced pressure;
The 3rd step: placed 2 ℃ of refrigerators static 6 hours, separate supernatant, using volume ratio is 1: 2 petroleum ether solution washing supernatant, organic solvent is removed in distilling under reduced pressure;
The 4th the step: adsorb with macroporous resin, adsorb saturated after, use the 2BV distilled water wash;
The 5th step: the eluant with containing 85% acetone carries out the eluting desorbing, and collects target product;
The 6th: target product obtains 0.15g Brown algae polyphenol solid after lyophilization, productive rate is 3 ‰.
Embodiment 3
Carry out the extraction of Brown algae polyphenol through following steps:
The first step: take by weighing the fresh Mus tail of 1000g algae, remove precipitate, phytoplankton and other attachment, rinse well repeatedly with tap water then, in 105 ℃ of baking ovens, dry to constant weight, obtain solid content and be about 50g, smash the refiner fragmentation to pieces with tissue;
Second step: the biological raw material after the fragmentation is pressed 2 of weight in wet base adding 0.004%; 6-di-t-butyl hydroxy-methylbenzene (BHT) and 0.004% sodium sulfite; With the mixed of the aqueous solution that contains methanol 50%, toluene 25% by 1: 3, fully stir to be placed on and handles 4min in the ultrasound wave, put into 50 ℃ of waters bath with thermostatic control, vibration, lucifuge leaching 3 hours; Separation of supernatant, organic solvent is removed in distilling under reduced pressure;
The 3rd step: placed 3 ℃ of refrigerators static 6 hours, separate supernatant, using volume ratio is 1: 1: 3 chloroform: petroleum ether: the solution washing supernatant of water, organic solvent is removed in distilling under reduced pressure;
The 4th the step: adsorb with macroporous resin, adsorb saturated after, use the 2BV distilled water wash;
The 5th step: use that to contain volume ratio be 2: 1: 2 methanol: ethyl acetate: the eluant solution desorbing of water, and collect target product;
The 6th step: target product obtains 0.125g Brown algae polyphenol solid after lyophilization, productive rate is 2.5 ‰.
The above is merely the preferred embodiments of the present invention, is not limited to the present invention, and for a person skilled in the art, the present invention can have various changes and variation.All within spirit of the present invention and principle, any modification of being done, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. the method for distilling of a Brown algae polyphenol is characterized in that: as raw material, carry out the operation of following steps with the biology that contains the Brown algae polyphenol:
Pretreatment of raw material: take by weighing the biological raw material that contains the Brown algae polyphenol of certain quantity of fresh, remove precipitate, phytoplankton and other attachment, rinse well repeatedly, dry, carry out fragmentation with tap water;
Leaching: with the antioxidant of the biomaterial after the fragmentation by weight in wet base adding 0.002～0.02%; With the aqueous solution that contains organic solvent 50～90% by 1: 2～9 mixed; Fully stir to be placed on and handle 3～6min in the ultrasound wave; Put into 40～80 ℃ of waters bath with thermostatic control, vibration, lucifuge leaching 1～6 hour, separate supernatant, organic solvent is removed in distilling under reduced pressure;
Cooling washing: will leach back solution and place 0～4 ℃ of refrigerator static 2～8 hours, separate supernatant, using volume ratio is that 1: 1～4 aqueous solutions of organic solvent wash supernatant, organic solvent is removed in distilling under reduced pressure;
Absorption: the solution that above-mentioned steps is obtained adsorbs with macroporous resin, adsorb saturated after, use the 2BV distilled water wash;
Eluting: the eluant with containing 50～85% organic solvents carries out the eluting desorbing, and collects target product;
Lyophilization: target product obtains finished product Brown algae polyphenol after lyophilization.
2. the method for distilling of Brown algae polyphenol according to claim 1 is characterized in that: the said biomaterial that contains the Brown algae polyphenol contains the thread of brown pigment or the thalloid algae of silk in life Yu Haiyang or the fresh water.
3. the method for distilling of Brown algae polyphenol according to claim 2 is characterized in that: the said biomaterial that contains the Brown algae polyphenol is Sargassum Brown algae or Larminaria plant.
4. the method for distilling of Brown algae polyphenol according to claim 1; It is characterized in that: the antioxidant that adds in the said leaching step is a butylated hydroxyarisol (BHA), 2, one or more in 6-di-t-butyl hydroxy-methylbenzene (BHT), sodium sulfite, sodium sulfite, sodium pyrosulfite, the sodium thiosulfate.
5. the method for distilling of Brown algae polyphenol according to claim 1 is characterized in that: the organic solvent of using in the said leaching step is one or more in acetone, methanol, toluene, ethanol, ethyl acetate, chloroform, the petroleum ether.
6. the method for distilling of Brown algae polyphenol according to claim 1 is characterized in that: the separation method of supernatant is siphon, centrifugal, in filtering one or more in the said leaching step.
7. the method for distilling of Brown algae polyphenol according to claim 1 is characterized in that: the organic solvent of using in the said cooling washing step is one or more in acetone, methanol, toluene, ethanol, ethyl acetate, chloroform, the petroleum ether.
8. the method for distilling of Brown algae polyphenol according to claim 1 is characterized in that: the organic solvent in the said elution step is one or more in ethanol, acetone, methanol, toluene, ethyl acetate, the chloroform.
9. the method for distilling of Brown algae polyphenol according to claim 1 is characterized in that: the Brown algae polyphenol finished product of said final acquisition is solid-state or liquid.
10. the method for distilling of Brown algae polyphenol according to claim 9 is characterized in that: the Brown algae polyphenol finished product of said final acquisition is solid-state.
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| CN2010102779021A CN102397300A (en) | 2010-09-10 | 2010-09-10 | Extraction method of phlorotannins |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103725034A (en) * | 2013-12-24 | 2014-04-16 | 上海海洋大学 | Method for extracting pigment from Sargassum horneri |
| CN104274496A (en) * | 2013-07-10 | 2015-01-14 | 山东洁晶集团股份有限公司 | Extraction method for sargassum horneri polyphenol |
| CN104824037A (en) * | 2015-05-18 | 2015-08-12 | 国家海洋局第三海洋研究所 | Method for preparing plant growth regulator containing products by using low-value seaweeds |
| DE102014105260A1 (en) * | 2014-04-14 | 2015-10-15 | CRM - Coastal Research & Management GbR (vertretungsberechtigter Gesellschafter: Dr. Levent Piker, 24159 Kiel) | cytostatic |
| CN106070339A (en) * | 2016-06-08 | 2016-11-09 | 北京大学深圳研究生院 | Brown algae polyphenols compositions with algistatic activity and its preparation method and application |
| CN107468718A (en) * | 2016-06-08 | 2017-12-15 | 北京大学深圳研究生院 | Marine algae extract, preparation method and use with antibacterial activity |
| CN108434177A (en) * | 2018-03-30 | 2018-08-24 | 中国农业科学院烟草研究所 | A kind of activity inhibitor and preparation method thereof and its in application hypoglycemic, in reducing blood lipid |
| CN113662112A (en) * | 2021-08-27 | 2021-11-19 | 大连工业大学 | Compound fruit and vegetable juice with eye protection function and preparation method thereof |
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| CN1202334A (en) * | 1998-05-28 | 1998-12-23 | 中国科学院海洋研究所 | Preparation of seeweed polyphenol antioxidation agent and its applying method |
| CN1715264A (en) * | 2004-07-02 | 2006-01-04 | 中国科学院海洋研究所 | A kind of method of from marine alga, extracting marine alga growth hormone |
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2010
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1202334A (en) * | 1998-05-28 | 1998-12-23 | 中国科学院海洋研究所 | Preparation of seeweed polyphenol antioxidation agent and its applying method |
| CN1715264A (en) * | 2004-07-02 | 2006-01-04 | 中国科学院海洋研究所 | A kind of method of from marine alga, extracting marine alga growth hormone |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104274496A (en) * | 2013-07-10 | 2015-01-14 | 山东洁晶集团股份有限公司 | Extraction method for sargassum horneri polyphenol |
| CN104274496B (en) * | 2013-07-10 | 2017-12-01 | 山东洁晶集团股份有限公司 | A kind of extracting method of Sargassum horneri polyphenol |
| CN103725034A (en) * | 2013-12-24 | 2014-04-16 | 上海海洋大学 | Method for extracting pigment from Sargassum horneri |
| CN103725034B (en) * | 2013-12-24 | 2015-05-27 | 上海海洋大学 | Method for extracting pigment from Sargassum horneri |
| DE102014105260A1 (en) * | 2014-04-14 | 2015-10-15 | CRM - Coastal Research & Management GbR (vertretungsberechtigter Gesellschafter: Dr. Levent Piker, 24159 Kiel) | cytostatic |
| CN104824037A (en) * | 2015-05-18 | 2015-08-12 | 国家海洋局第三海洋研究所 | Method for preparing plant growth regulator containing products by using low-value seaweeds |
| CN106070339A (en) * | 2016-06-08 | 2016-11-09 | 北京大学深圳研究生院 | Brown algae polyphenols compositions with algistatic activity and its preparation method and application |
| CN107468718A (en) * | 2016-06-08 | 2017-12-15 | 北京大学深圳研究生院 | Marine algae extract, preparation method and use with antibacterial activity |
| CN106070339B (en) * | 2016-06-08 | 2019-04-19 | 北京大学深圳研究生院 | Brown algae polyphenols composition with algistatic activity and its preparation method and application |
| CN107468718B (en) * | 2016-06-08 | 2021-03-09 | 北京大学深圳研究生院 | Seaweed extract with antibacterial activity, preparation method and application thereof |
| CN108434177A (en) * | 2018-03-30 | 2018-08-24 | 中国农业科学院烟草研究所 | A kind of activity inhibitor and preparation method thereof and its in application hypoglycemic, in reducing blood lipid |
| CN113662112A (en) * | 2021-08-27 | 2021-11-19 | 大连工业大学 | Compound fruit and vegetable juice with eye protection function and preparation method thereof |
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Application publication date: 20120404 |